In the manufacture of a thin film metal alloy or metal oxide magnetic recording disk, a fluoroether lubricant is bonded to the carbon or hydrogenated carbon overcoat of the disk. The lubricant is applied to the carbon overcoat by dipping the disk in a solution of the lubricant. The lubricated disk is then exposed to the plasma of an inert gas, such as nitrogen. The resulting disk contains a layer of lubricant which is bonded to the disk surface so as to be resistant to spin-off and which has a relatively uniform thickness so as to substantially eliminate the problems of stiction during the operation of the disk file.

Patent
   4960609
Priority
Nov 13 1989
Filed
Nov 13 1989
Issued
Oct 02 1990
Expiry
Nov 13 2009
Assg.orig
Entity
Large
37
4
EXPIRED
1. A process for bonding a fluoroether lubricant to a thin film magnetic recording disk of the type having a protective overcoat consisting essentially of carbon, the process comprising the steps of:
applying a fluoroether lubricant to the carbon overcoat surface; and
thereafter exposing the lubricated disk to a plasma of an essentially inert gas.
2. The process according to claim 1 wherein the step of exposing the lubricated disk to an essentially inert gas plasma comprises the step of exposing the lubricated disk to a nitrogen gas plasma.
3. The process according to claim 1 wherein the step of applying the fluoroether lubricant comprises the step of dipping the carbon overcoated disk into a solution containing the fluoroether lubricant.
4. The process according to claim 1 further comprising the step of, after exposing the lubricated disk to the plasma, removing the unbonded lubricant from the disk.
5. The process according to claim 1 wherein the step of applying the fluoroether lubricant comprises the step of applying a difunctional derivative of a perfluoropolyether lubricant.
6. The process according to claim 1 wherein the step of applying the fluoroether lubricant comprises the step of applying a non-reactive perfluoropolyether lubricant.

This invention relates to a process for the manufacture of a thin film metal alloy or metal oxide magnetic recording disk, and in particular to a process for the bonding of a liquid lubricant to the carbon protective overcoat on the disk.

Thin film magnetic recording disks typically comprise a substrate, such as an aluminum-magnesium (AlMg) alloy with a nickel-phosphorous (NiP) surface coating, a magnetic film of either a cobalt based metal alloy or a gamma iron oxide film, and a protective overcoat, such as a sputter-deposited amorphous carbon or hydrogenated carbon film, formed over the magnetic layer. A liquid lubricant, such as a fluoroether lubricant, is often applied to the carbon or hydrogenated carbon overcoat. A general description of the structure of such thin film disks is given in U.S. Pat. Nos. 4,610,911 to Opfer, et al., and 4,552,820 to Lin, et al. An amorphous film for use as a protective overcoat is described in U.S. Pat. Nos. 4,503,125 to Nelson, et al. and an amorphous hydrogenated carbon film is described in assignee's U.S. Pat. No. 4,778,582 to Howard.

There are several problems with such disks which are caused essentially by the liquid lubricant on the protective overcoat. In particular, because there is no means to specifically retain the liquid lubricant onto the overcoat, the lubricant tends to deplete due to spin-off during operation of the disk file. In addition, variations in thickness of the lubricant over the disk surface can cause problems in operation of the disk file. If the lubricant layer is too thin the air bearing slider which supports the read/write head can cause wear of the disk surface. If the lubricant layer is too thick the slider can become stuck to the disk surface when the disk file is turned off. This static friction or "stiction" is caused by a variety of factors, including viscous shear forces and surface tension created by the lubricant between the protective overcoat and the slider. This stiction can result in damage to the head or disk when the slider suddenly breaks free from the disk surface when disk rotation is initiated. Also, because the suspension which supports the slider is relatively fragile in order to permit the slider to "fly" above the disk surface, sudden rotation of the disk in the presence of stiction can also damage the suspension.

The present invention is a process for grafting or bonding the fluoroether lubricant to the carbon or hydrogenated carbon protective overcoat. The fluoroether lubricant is first applied to the disk and thereafter exposed to a plasma of an essentially inert gas. The plasma exposure bonds the lubricant to the carbon overcoat. The lubricant which is bonded to the carbon overcoat by the plasma treatment is resistant to spin-off and has a thickness uniformity which substantially eliminates the occurrence of stiction during operation of the disk file.

For a fuller understanding of the nature and advantages of the present invention reference should be made to the following detailed description.

The lubricants were applied to the carbon overcoat surfaces of the disks from dilute solutions of the liquid lubricants in 1,1,2-trichlorotrifluoroethane (Freon). The lubricants were applied to the various disks by either dipping, evaporation, spin coating or wiping. The lubricants used were the perfluoropolyethers (PFPE), i.e., Fomblin Z and Y lubricants made by Montedison, Krytox made by Dupont and Demnum made by Daikin, and their difunctional derivatives containing various reactive end groups, e.g., hydroxyl (Fomblin Z-DOL), piperonyl (Fomblin AM2001), and isocyanate (Fomblin Z-DISOC), all manufactured by Montedison. The difunctional derivatives are referred to as reactive fluoroether lubricants. The chemical structures of the lubricants are given in Table 1.

TABLE 1
__________________________________________________________________________
STRUCTURE OF PERFLUOROETHER LUBRICANTS
Lubricant Formula
__________________________________________________________________________
Fomblin Z-25
CF3 O(CF2 CF2 O)n(CF2 O)mCF3
Fomblin Z-15
CF3 O(CF2 CF2 O)n(CF2 O)mCF3
Fomblin Z-03
CF3 O(CF2 CF2 O)n(CF2 O)mCF3
Fomblin Z-DOL
HOCH2 CF2 O(CF2 CF2 O)n(CF2 O)mCF
2 CH2 OH
Fomblin AM2001
Piperonyl-OCH2 CF2 O(CF2 CF2 O)n(CF2
O)mCF2 CH2 O-piperonyl1
Fomblin Z-DISOC
OCNC6 H3 (CH3)NHCOCF2 O(CF2 CF2
O)n(CF2 O)mCF2CONHC6 H3 (CH3)NCO
Fomblin YR
##STR1##
Demnum F(CF2 CF2 CF2 O)nCF2 CF3
Krytox
##STR2##
__________________________________________________________________________
1 3,4-methylenedioxybenzyl

In the dipping process, the thickness of the lubricant coating is determined by controlling the withdrawal speed and the concentration of lubricant in the solution. The lubricant layer thickness is also sensitive to lubricant type, the surface of the substrate and the ambient conditions.

After the disks were lubricated in this manner, plasma treatments were carried out by exposure of the lubricated carbon surfaces of the disks to a nitrogen (N2) plasma for 2 to 5 minutes in a LFE plasma system operating at 13.6 MHz. Nitrogen gas of purity 99.999% was used without further purification at a flow rate of 20 cc/min, with the pressure maintained at 0.2 torr. The disk samples were placed horizontally in the plasma chamber. After plasma treatment the unbonded component of the lubricant was removed by thoroughly washing the disks with Freon.

Nitrogen plasma grafting of fluoroether lubricants to the surface of the carbon overcoat was demonstrated with both non-reactive and reactive lubricants using powers in the range of 20 W to 250 W. It was found that the level of lubricant attachment to the carbon overcoat varies considerably with plasma power and time of exposure for a fixed initial lubricant thickness. Table 2 is a comparison of lubricant thicknesses, after irradiation of 30 Å of Z-DOL on the carbon overcoat surfaces with a nitrogen plasma for 2 minutes at different powers, with lubricant thicknesses after Freon rinse.

TABLE 2
______________________________________
EFFECT OF ROOM TEMPERATURE
N2 PLASMA ON 30 Å Z-DOL
Thickness Thickness
Plasma After Plasma
After
Conditions Treatment (Å)
Freon Rinse (Å)
______________________________________
None 30 0
20 Watt/2 min
25 18
50 Watt/2 min
23 15
75 Watt/2 min
15 10
100 Watt/2 min
5 2
______________________________________

Lubricant thickness measurements were made by a X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared analysis (FTIR). As clearly shown by the data in Table 2, the plasma treatment enhances the adhesion of the lubricant to the surface of the carbon overcoat.

In the experimental results described above, the disks with the bonded lubricant were thereafter washed in Freon to remove any unbonded lubricant. However, it is possible in the manufacturing of the disks to control the thickness of the lubricant applied during the dipping process, such that following plasma treatment it is not necessary to remove unbonded lubricant. While the disks used in these experimental results contained a hydrogenated carbon overcoat (i.e. an essentially carbon overcoat containing less than 20 atomic percent hydrogen), the process is fully applicable for disks having an essentially amorphous carbon film without substantial hydrogen present since it is believed that the lubricant is bonded to carbon atoms in the overcoat. The preferred inert gas is N2. However, other gases which are "inert", i.e. essentially not chemically reactive with the fluoroether lubricant or the carbon overcoat, would also be suitable in the present process. An example of such a gas is argon. In the experiment described above, a reactive lubricant, Z-Dol, with difunctional end groups is used. If a non-functional lubricant is used, such as Fomblin Z-15 or YR made by Montedison, essentially the same results are obtained except that the power and exposure time are somewhat larger to produce the optimal bonding.

While the preferred embodiment of the present invention has been described in detail, it should be apparent to those skilled in the art that modifications and adaptations to that embodiment may occur to one skilled in the art without departing from the scope of the present invention as set forth in the following claims.

Homola, Andrew M., Saperstein, David D., Lin, Li-Ju J.

Patent Priority Assignee Title
5030478, Mar 03 1989 MARIANA HDD B V ; HITACHI GLOBAL STORAGE TECHNOLOGIES NETHERLANDS B V Process for bonding lubricants to thin film recording media
5049410, Nov 01 1989 International Business Machines Corporation Lubricant film for a thin-film disk
5227211, Apr 21 1989 WD MEDIA, INC Magnetic recording disk medium comprising a magnetic thin film and a carbon overcoat having surface nitrogen atoms, a specified carbon structure, and oxygen atoms
5525392, Dec 10 1992 International Business Machines Corporation Magnetic recording medium having a fluorinated polymeric protective layer formed by an ion beam
5543203, Aug 06 1993 Hitachi Global Storage Technologies Japan, Ltd Magnetic recording medium having a protective layer which includes high and low surface energy regions and a lubricant
5559650, Nov 13 1992 Seagate Technology LLC Lubricated disk drive
5562965, Jun 07 1995 Seagate Technology LLC Vapor lubrication of fractionated lubricant on thin film discs
5591481, Jul 15 1991 Matsushita Electric Industrial Co., Ltd. Method of manufacturing a magnetic recording medium including forming a graft polymer lubricant layer by irradiating monomers with radicals or atomic gas
5661618, Dec 11 1995 MARIANA HDD B V ; HITACHI GLOBAL STORAGE TECHNOLOGIES NETHERLANDS B V Magnetic recording device having a improved slider
5741577, Nov 10 1994 Kao Corporation Magnetic recording medium having a lubricant layer with a specified structure of a specified perfluoropolyether lubricant
5858536, Aug 25 1993 NEC Corporation Magnetic recording medium having a perfluoropolyether lubricant bonded to the surface of a carbon protective film
5900288, Jan 03 1994 Xerox Corporation Method for improving substrate adhesion in fluoropolymer deposition processes
5922415, Jun 18 1997 Southwest Research Institute Lubrication of magnetic disk storage media
6001479, May 30 1995 FUJI ELECTRIC DEVICE TECHNOLOGY CO , LTD Magnetic recording medium and method for manufacturing the same
6035681, Mar 12 1997 MARIANA HDD B V ; HITACHI GLOBAL STORAGE TECHNOLOGIES NETHERLANDS B V Etched/lubricated swage balls for use in DASD suspension-arm
6110330, Jun 28 1999 Trace Storage Technology Corp Process for bonding lubricant to magnetic disk
6122143, Feb 24 1989 NASH, JEFFREY M AS REPRESENTATIVE, AND FOR THE BENEFIT, OF THE FORMER Wet rigid disk drive assembly with a conical spindle bearing
6132875, Sep 12 1993 Showa Denko K K Magnetic recording medium and magnetic head having carbon protective layers
6183831, Aug 20 1998 Intevac, Inc.; Intevac, Inc Hard disk vapor lube
6379801, Dec 07 1998 Seagate Technology LLC Silane derivatized lubricants for magnetic recording media
6410103, Jul 24 1998 Showa Denko K K Memory disc, manufacturing method thereof, and method of manufacturing disc drive utilizing such memory disc
6551703, Dec 07 1998 Seagate Technology LLC Silane derivatized lubricants for magnetic recording media
6589641, Jun 04 1998 Seagate Technology LLC Thin films of crosslinked fluoropolymer on a carbon substrate
6617011, May 07 1999 Seagate Technology LLC Elastomeric lubricants for magnetic recording media
6627302, Mar 27 2001 Seagate Technology LLC Lubricant overcoat for recording media and a process for making the same
6680079, Jun 02 2000 Seagate Technology LLC Planarization and corrosion protection of patterned magnetic media
6821627, Jun 02 2000 Seagate Technology LLC Planarization and corrosion protection of patterned magnetic media
6849304, Mar 16 2001 Seagate Technology LLC Method of forming lubricant films
6861102, May 07 1999 Seagate Technology LLC Elastomeric lubricants for magnetic recording media
7431989, May 06 2003 TRIBOFILM RESEARCH, INC Article with lubricated surface and method
7553529, May 06 2003 TriboFilm Research, Inc. Article with lubricated surface and method
7674504, May 06 2003 Article with lubricated surface and method
8084103, Aug 15 2006 TRIBOFILM RESEARCH, INC Method for treating a hydrophilic surface
8124207, Mar 02 2004 TRIBOFILM RESEARCH, INC Article with lubricated surface and method
9133412, Jul 09 2012 TRIBOFILM RESEARCH, INC Activated gaseous species for improved lubrication
9315757, Jul 09 2012 TriboFilm Research, Inc. Activated gaseous species for improved lubrication
9984715, Sep 30 2008 Western Digital Technologies, INC Magnetic disk and manufacturing method thereof
Patent Priority Assignee Title
4503125, Oct 01 1979 Xebec, Inc. Protective overcoating for magnetic recording discs and method for forming the same
4552820, Apr 25 1984 Lin Data Corporation Disc media
4610911, Nov 03 1983 Hewlett-Packard Company Thin film magnetic recording media
4778582, Jun 02 1987 International Business Machines Corporation; INTERNATIONAL BUSINESS MACHINES CORPORATION, ARMONK, NEW YORK 10504, A CORP OF NEW YORK Process for making a thin film metal alloy magnetic recording disk with a hydrogenated carbon overcoat
////
Executed onAssignorAssigneeConveyanceFrameReelDoc
Nov 10 1989HOMOLA, ANDREW M International Business Machines CorporationASSIGNMENT OF ASSIGNORS INTEREST 0051740982 pdf
Nov 10 1989LIN, LI-JU J International Business Machines CorporationASSIGNMENT OF ASSIGNORS INTEREST 0051740982 pdf
Nov 10 1989SAPERSTEIN, DAVID D International Business Machines CorporationASSIGNMENT OF ASSIGNORS INTEREST 0051740982 pdf
Nov 13 1989International Business Machines Corporation(assignment on the face of the patent)
Date Maintenance Fee Events
Jan 24 1994M183: Payment of Maintenance Fee, 4th Year, Large Entity.
Apr 28 1998REM: Maintenance Fee Reminder Mailed.
Oct 04 1998EXP: Patent Expired for Failure to Pay Maintenance Fees.


Date Maintenance Schedule
Oct 02 19934 years fee payment window open
Apr 02 19946 months grace period start (w surcharge)
Oct 02 1994patent expiry (for year 4)
Oct 02 19962 years to revive unintentionally abandoned end. (for year 4)
Oct 02 19978 years fee payment window open
Apr 02 19986 months grace period start (w surcharge)
Oct 02 1998patent expiry (for year 8)
Oct 02 20002 years to revive unintentionally abandoned end. (for year 8)
Oct 02 200112 years fee payment window open
Apr 02 20026 months grace period start (w surcharge)
Oct 02 2002patent expiry (for year 12)
Oct 02 20042 years to revive unintentionally abandoned end. (for year 12)